HRID1179478

反应详情

EQUATION

反应方程式

HRID 1179478 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Lithium bis(trimethylsilyl) amide (1.0 M solution in tetrahydrofuran, 542 mL, 0.542 mol) was added to a solution of 3,5-difluoroaniline (35 g, 0.271 mol) in THF (60 mL) at 0° C. Isopropyl chloroformate (1M solution in toluene, 406 mL, 0.406 mol) was then added dropwise at 0° C. and the mixture allowed to warm to room temperature over 2 h. The reaction mixture was diluted with ether and washed with 1N hydrochloric acid, water, saturated aqueous sodium bicarbonate, brine and dried (MgSO4). Solvent was removed under vacuum and the residue was triturated in hexanes to obtain the title compound.

WORKUP

后处理

  1. washwashed with 1N hydrochloric acid, water, saturated aqueous sodium bicarbonate, brine
  2. dry with materialdried (MgSO4)
  3. customSolvent was removed under vacuum
  4. customthe residue was triturated in hexanes